CN108557881A - A kind of method of bismuth-containing material production high-purity bismuth oxide - Google Patents
A kind of method of bismuth-containing material production high-purity bismuth oxide Download PDFInfo
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- CN108557881A CN108557881A CN201810034185.6A CN201810034185A CN108557881A CN 108557881 A CN108557881 A CN 108557881A CN 201810034185 A CN201810034185 A CN 201810034185A CN 108557881 A CN108557881 A CN 108557881A
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- bismuth
- containing material
- solution
- purity
- bismuth oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods that bismuth-containing material produces high-purity bismuth oxide, first, bismuth-containing material and hydrochloric acid solution are carried out Leach reaction so that the bismuth in bismuth-containing material is entered in the form of bismuth chloride in solution, isolates leachate and leached mud；Then, pure water is added into leachate, bismuth chloride occurs hydrolysis and is settled out chlorine oxygen bismuth；Then, precipitation chlorine oxygen bismuth is isolated, and dilute alkaline soln is added, chlorine oxygen bismuth is converted to bismuth hydroxide under conditions of low temperature diluted alkaline；Concentrated alkali solution is added into filtered bismuth hydroxide again, bismuth oxide is converted to by high-temperature concentrated alkali；Finally, the bismuth oxide of generation is washed, is dried, sieved and can be obtained the high-purity bismuth oxide.The present invention makes bismuth enter solution in the form of bismuth chloride using bismuth-containing material as raw material, then is hydrolyzed into chlorine oxygen bismuth, is converted by the conversion of low temperature diluted alkaline, high-temperature concentrated alkali, generates bismuth oxide.This method flow is simple, and reagent consumption is few, the impurity such as energy deep purifying separation Fe, Pb, Sb, As.
Description
Technical field
The present invention relates to the production technical field of bismuth oxide, more particularly to a kind of side of bismuth-containing material production high-purity bismuth oxide
Method.
Background technology
Bismuth oxide is the important source material in light industry, chemical industry, ceramics, electronic component and medical industry, and it is high to be also applied for manufacture
Index of refraction glass, nuclear industry glass and nuclear reactor fuel etc..The method of traditional mode of production bismuth oxide be using refined bismuth as raw material,
It after nitrifying the bismuth nitrate tinning that condensing crystallizing comes out, is put into calcining furnace, at a temperature of 500~600 DEG C, calcines denitration,
Crushing can be obtained bismuth oxide product.Due to having a large amount of toxic gas during directly preparing bismuth oxide from bismuth nitrate calcining
NOXIt overflows, causes the pollution of air, therefore, to being directly improved with bismuth nitrate calcine technology, make bismuth nitrate and ammonium bicarbonate or ammonia
Water reaction is converted to bismuthyl carbonate, basic bismuth nitrate or bismuth hydroxide, then is calcined.But due to the intermediate production in conversion process
Composition granule is thinner, large specific surface area, and the absorption of precipitation and package phenomenon are serious, will cause the washing difficulty of precipitation and calcined
Inevitably still there is part toxic gas NO in journeyXIt overflows.Therefore, traditional mode of production energy consumption is big, and there are a large amount of toxic gases in when calcining
It overflows, such as handles, air will be polluted, it is big that there are equipment investments, the high problem of production cost without absorption.
Invention content
Based on the production procedure that solves bismuth oxide in the prior art is long, process is complicated, of high cost and carcinogenic substance NOXIt is right
The big caused problem of pollution of environment, the application propose that a kind of method of bismuth-containing material production high-purity bismuth oxide, energy depth are net
Change the impurity such as separation Fe, Pb, Sb, As.
The purpose of the present invention will be achieved through the following technical solutions：A kind of method of bismuth-containing material production high-purity bismuth oxide,
It comprises the following processes：First, bismuth-containing material and hydrochloric acid solution are subjected to Leach reaction so that the bismuth in bismuth-containing material is with bismuth chloride
Form enter in solution, isolate leachate and leached mud；Then, pure water is added into leachate, water occurs for bismuth chloride
Solution reaction is settled out chlorine oxygen bismuth；Then, precipitation chlorine oxygen bismuth is isolated, and dilute alkaline soln is added, item of the chlorine oxygen bismuth in low temperature diluted alkaline
It is converted to bismuth hydroxide under part；Concentrated alkali solution is added into filtered bismuth hydroxide again, bismuth hydroxide turns by high-temperature concentrated alkali
It is melted into bismuth oxide；Finally, the bismuth oxide of generation is washed, is dried, sieved and can be obtained the high-purity bismuth oxide.
Preferably, a kind of method of bismuth-containing material production high-purity bismuth oxide, the bismuth-containing material bismuth-containing grade exist
Between 10~20%.
Preferably, the method for described a kind of bismuth-containing material production high-purity bismuth oxide, the hydrochloric acid solution it is a concentration of
The liquid-solid ratio 5 of 150g/L, hydrochloric acid solution and bismuth-containing material：1(mL/g).
Preferably, the method for a kind of bismuth-containing material production high-purity bismuth oxide, the bismuth-containing material and hydrochloric acid solution
The time for carrying out Leach reaction is 2h, while mechanical agitation, speed of agitator are 200 revs/min.
Preferably, the method for described a kind of bismuth-containing material production high-purity bismuth oxide, when the hydrolysis, using go from
Leachate is diluted to original 5 times by sub- water, will be precipitated out after chlorine oxygen bismuth stands 2~3 hours and is separated by filtration.
Preferably, the method for a kind of bismuth-containing material production high-purity bismuth oxide, the dilute alkaline soln and chlorine oxygen bismuth
Liquid-solid ratio is 3：1 (mL/g), reaction temperature are 20~60 DEG C (room temperature), reaction time 2h.
Preferably, the method for a kind of bismuth-containing material production high-purity bismuth oxide, the dilute alkaline soln are sodium hydroxide
Solution, a concentration of 60g/L of sodium hydroxide solution.
Preferably, the method for a kind of bismuth-containing material production high-purity bismuth oxide, the concentrated alkali solution and bismuth hydroxide
Liquid-solid ratio be 3：1 (mL/g), reaction temperature are 100 DEG C, reaction time 1h.
Preferably, the method for a kind of bismuth-containing material production high-purity bismuth oxide, the concentrated alkali solution are sodium hydroxide
Solution, a concentration of 240g/L of sodium hydroxide solution.
Preferably, a kind of method of bismuth-containing material production high-purity bismuth oxide, the bismuth oxide use the hydrogen of 10g/L
Sodium hydroxide solution is washed, and is put into after washing and is dried into electric dry oven, and the control of the temperature of the electric dry oven is at 100~110 DEG C, the bed of material
Thickness be 40~50mm, smashed after dry 5~6h, cross 200 mesh sieve and can be obtained high-purity bismuth oxide.
Compared with prior art, beneficial effects of the present invention：The present invention directly using bismuth-containing material as raw material, makes bismuth with chlorination
The form of bismuth enters solution, then is hydrolyzed into chlorine oxygen bismuth, is converted by the conversion of low temperature diluted alkaline, high-temperature concentrated alkali, generates oxidation
Bismuth.This method flow is simple, and reagent consumption is few, the impurity such as energy deep purifying separation Fe, Pb, Sb, As.
Description of the drawings
Fig. 1 is the flow chart for the method that a kind of bismuth-containing material of the present invention produces high-purity bismuth oxide.
Specific implementation mode
To more fully understand the present invention, further specific elaboration is made to the present invention below by following embodiment, but not
Limitation of the invention is can be regarded as, some are nonessential according to made by foregoing invention content for those skilled in the art
It improves and adjusts, be also considered as being within the scope of the present invention.
Embodiment 1
A kind of method of bismuth-containing material production high-purity bismuth oxide, comprises the following processes：
Leaching process：Bismuth-containing material and hydrochloric acid solution are subjected to Leach reaction, a concentration of 150g/L of hydrochloric acid, liquid-solid ratio 5：
1 (mL/g), the Leach reaction time is 2h, while mechanical agitation, speed of agitator are 200 revs/min, and the bismuth in bismuth-containing material is with chlorination
The form of bismuth enters in solution；
Hydrolytic process：Deionized water is added into solution, solution is diluted to original 5 times, it is anti-that hydrolysis occurs for bismuth chloride
It should be settled out chlorine oxygen bismuth, chlorine oxygen bismuth precipitation is filtered out after standing 2~3h；
Low temperature diluted alkaline converts：Diluted alkaline is added into the chlorine oxygen bismuth precipitation isolated, diluted alkaline is sodium hydroxide solution, hydroxide
A concentration of 60g/L of sodium solution, liquid-solid ratio 3：1 (mL/g), reaction temperature are 60 DEG C, reaction time 2h, and chlorine oxygen bismuth is herein
Under the conditions of be converted to bismuth hydroxide；
High-temperature concentrated alkali converts：Filtered bismuth hydroxide is reacted with concentrated base again, concentrated base is sodium hydroxide solution, hydroxide
A concentration of 240g/L of sodium solution, reaction temperature are 100 DEG C, liquid-solid ratio 3：1 (mL/g), reaction time 1h, at this time hydrogen-oxygen
Change bismuth and is converted to bismuth oxide；
Post-processing：The bismuth oxide of generation is washed using the sodium hydroxide solution of 10g/L, is put into electric dry oven after washing
Drying, at 100~110 DEG C, the thickness of the bed of material is 40~50mm, is smashed after 5~6 hours dry, mistake for the temperature control of electric dry oven
200 mesh sieve can be obtained high-purity bismuth oxide.
The foregoing is merely illustrative of the preferred embodiments of the present invention, but does not limit the protection content of the present invention, all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention.
Claims (10)
1. a kind of method of bismuth-containing material production high-purity bismuth oxide, which is characterized in that comprise the following processes：First, by bismuth-containing object
Material carries out Leach reaction with hydrochloric acid solution so that the bismuth in bismuth-containing material is entered in the form of bismuth chloride in solution, is isolated
Leachate and leached mud；Then, pure water is added into leachate, bismuth chloride occurs hydrolysis and is settled out chlorine oxygen bismuth；Then, divide
Precipitation chlorine oxygen bismuth is separated out, and dilute alkaline soln is added, chlorine oxygen bismuth is converted to bismuth hydroxide under conditions of low temperature diluted alkaline；Again to filtering
Concentrated alkali solution is added in bismuth hydroxide afterwards, bismuth hydroxide is converted to bismuth oxide by high-temperature concentrated alkali；Finally, the bismuth oxide of generation
It washed, dried, sieved and can be obtained the high-purity bismuth oxide.
2. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The bismuth-containing
Material bismuth-containing grade is between 10~20%.
3. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The hydrochloric acid
The liquid-solid ratio 5 of a concentration of 150g/L of solution, hydrochloric acid solution and bismuth-containing material：1(mL/g).
4. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The bismuth-containing
The time that material carries out Leach reaction with hydrochloric acid solution is 2h, while mechanical agitation, speed of agitator are 200 revs/min.
5. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The hydrolysis
When reaction, leachate is diluted to by original 5 times using deionized water, will be precipitated out after chlorine oxygen bismuth stands 2~3 hours and filter
Separation.
6. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The diluted alkaline
The liquid-solid ratio of solution and chlorine oxygen bismuth is 3：1 (mL/g), reaction temperature are 20~60 DEG C, reaction time 2h.
7. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The diluted alkaline
Solution is sodium hydroxide solution, a concentration of 60g/L of sodium hydroxide solution.
8. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The concentrated base
The liquid-solid ratio of solution and bismuth hydroxide is 3：1 (mL/g), reaction temperature are 100 DEG C, reaction time 1h.
9. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The concentrated base
Solution is sodium hydroxide solution, a concentration of 240g/L of sodium hydroxide solution.
10. a kind of method of bismuth-containing material production high-purity bismuth oxide according to claim 1, it is characterised in that：The oxygen
Change bismuth to wash using the sodium hydroxide solution of 10g/L, is put into after washing and is dried into electric dry oven, the temperature control of the electric dry oven
At 100~110 DEG C, the thickness of the bed of material is 40~50mm, is smashed after dry 5~6h, crosses 200 mesh sieve and can be obtained high pure zirconia
Bismuth.
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| CN201810034185.6A CN108557881B (en) | 2018-01-15 | 2018-01-15 | Method for producing high-purity bismuth oxide from bismuth-containing material |
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| CN201810034185.6A CN108557881B (en) | 2018-01-15 | 2018-01-15 | Method for producing high-purity bismuth oxide from bismuth-containing material |
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| CN108557881B CN108557881B (en) | 2020-07-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180649A (en) * | 2022-08-25 | 2022-10-14 | 中南大学 | Method for preparing high-purity bismuth oxychloride from molybdenum-bismuth sulfide ore |
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| JPH035323A (en) * | 1989-06-02 | 1991-01-11 | Sumitomo Metal Mining Co Ltd | Production of fine bismuth oxide |
| CN1433969A (en) * | 2002-01-24 | 2003-08-06 | 吴世军 | Production process for regular system high-purity bismuth oxide |
| CN1544337A (en) * | 2003-11-25 | 2004-11-10 | 中南大学 | Nanometer bismuth oxide preparation process |
| CN101811732A (en) * | 2009-12-23 | 2010-08-25 | 株洲冶炼集团股份有限公司 | Superfine and high-purity bismuth oxide and preparation method thereof |
| CN102180517A (en) * | 2011-03-17 | 2011-09-14 | 云南祥云飞龙有色金属股份有限公司 | Method for producing dibismuth trioxide by using bismuth oxychloride |
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| JPH035323A (en) * | 1989-06-02 | 1991-01-11 | Sumitomo Metal Mining Co Ltd | Production of fine bismuth oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180649A (en) * | 2022-08-25 | 2022-10-14 | 中南大学 | Method for preparing high-purity bismuth oxychloride from molybdenum-bismuth sulfide ore |
| CN115180649B (en) * | 2022-08-25 | 2023-10-27 | 中南大学 | Method for preparing high-purity bismuth oxychloride from molybdenum bismuth sulfide ore |
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| CN108557881B (en) | 2020-07-28 |
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